CN114481288A - SiC support holder for growing crucible in tellurium-zinc-cadmium crystal preparation process - Google Patents

SiC support holder for growing crucible in tellurium-zinc-cadmium crystal preparation process Download PDF

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Publication number
CN114481288A
CN114481288A CN202011156052.XA CN202011156052A CN114481288A CN 114481288 A CN114481288 A CN 114481288A CN 202011156052 A CN202011156052 A CN 202011156052A CN 114481288 A CN114481288 A CN 114481288A
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crystal
growth crucible
growth
base body
arc
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CN114481288B (en
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赵鹏
姜军
孔金丞
陈少璠
赵文
庹梦寒
袁绶章
王静宇
姬荣斌
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Kunming Institute of Physics
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002Crucibles or containers for supporting the melt
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/46Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention relates to a SiC support holder for a growth crucible in a tellurium-zinc-cadmium crystal preparation process, which comprises a base substrate, wherein the base substrate is a cylindrical growth crucible support holder, the upper end surface of the base substrate is an arc-shaped groove matched with the bottom surface of the growth crucible in shape, the outer diameter of a circle where the arc of the section of the arc-shaped groove is located is the same as the outer diameter of an equal-diameter section of the growth crucible, the inner diameter of the circle is slightly larger than the outer diameter of a seed crystal part of the growth crucible and is filled with SiC powder, and the concave surface of the arc-shaped groove and the outer side of the base substrate are in fillet transition. A cylinder concentric with the base body is dug out from the lower end face of the base body and is used for being nested at the top end of a crystal growing rod for crystal growth, and the crystal can be guaranteed to be stable in the middle of a growth furnace. The length of the base body is the same as that of the equal-diameter part of the growth crucible. In the process of growing the CdZnTe crystal, the invention extracts the heat in the CdZnTe crystal in time, helps to establish ideal crystal growth thermal field conditions, stabilizes the form of a solid-liquid interface and greatly improves the quality and the single crystal rate of the CdZnTe single crystal.

Description

SiC support holder for growing crucible in tellurium-zinc-cadmium crystal preparation process
Technical Field
The invention relates to the field of crystal preparation, in particular to a SiC support for a growth crucible in a tellurium-zinc-cadmium crystal preparation process.
Background
As is well known, in the process of growing single crystals by a solution method, the control of the shape and stability of a solid-liquid interface is the core of a single crystal growing process, and the key point of obtaining complete single crystals and improving the crystal quality is whether a favorable and stable solid-liquid interface can be obtained or not. The shape of the solid-liquid interface is mainly determined by the heat transportation condition in the crystal growth process. The heat transport at the solid-liquid interface mainly includes heat exchange with a high temperature region, heat exchange with a low temperature region, and heat exchange with the surrounding environment. Therefore, controlling the heat transport at the solid-liquid interface, providing a suitable and stable temperature field, is very important in the process of growing single crystals by the solution method.
The heat transport at the solid-liquid interface is divided into two vector directions, one axial, called axial heat flow (QC), and the other radial, called radial heat flow (QR). In the process of growing single crystals by the solution method, an ideal solid-liquid interface is a flat solid-liquid interface without radial heat flow and only with axial heat flow, or the radial heat flow is a convex solid-liquid interface transported to the crystal from the surrounding environment.
However, in the growing process of the tellurium-zinc-cadmium crystal, as the solid thermal conductivity is lower than the liquid thermal conductivity, the axial thermal flow is continuously reduced and the radial thermal flow is continuously enhanced along with the rising of the growing solid-liquid interface, and the shape and the stability of the solid-liquid interface are influenced, so that the tellurium-zinc-cadmium crystal becomes a concave liquid surface which is not beneficial to the growth of single crystals. Meanwhile, the unstable solid-liquid interface is easy to induce new crystal nuclei in the growth process of the crystal, so that the crystal defects are increased.
Disclosure of Invention
The invention aims to provide a SiC support holder of a growth crucible, which enables the shape of a solid-liquid interface to be more stable in the preparation process of a cadmium zinc telluride crystal.
The technical scheme adopted by the invention is as follows:
the utility model provides a SiC supports and holds in palm that is used for tellurium zinc cadmium crystal preparation in-process growth crucible, includes the base member, the base member support for the cylinder growth crucible that the SiC material was prepared holds in the palm, is the cylinder shape, the up end of base member is the cambered surface recess anastomotic with growth crucible bottom surface shape, the external diameter of cambered surface recess cross-section arc place circle is the same with the external diameter of growth crucible constant diameter section, the internal diameter ratio is slightly bigger than the seed crystal part external diameter of growth crucible, cambered surface recess concave surface becomes the fillet transition with the outside of base member. A cylinder concentric with the base body is dug out from the lower end surface of the base body and is used for being nested at the top end of a long crystal rod for crystal growth. The length of the base body is the same as that of the equal-diameter part of the growth crucible.
Further, the base substrate is cylindrical.
Further, the SiC support is suitable for growing the cadmium zinc telluride single crystal by a vertical Bridgman method (VB) and a vertical temperature gradient freezing method (VGF).
The working principle of the invention is as follows:
the SiC support with the cylindrical body concentric with the base body dug out is nested at the top end of a long crystal rod of the tellurium-zinc-cadmium crystal body, the outer diameter of the long crystal rod is the same as that of the cylindrical body, and the shaking effect is avoided in the crystal growth process. Because the outer diameter of the arc-shaped circle of the arc-shaped groove interface is the same as the outer diameter of the growth crucible, and the shape of the arc-shaped groove 2 is completely matched with the shape of the bottom surface of the growth crucible, the contact area of the arc-shaped groove 2 and the outer wall of the growth crucible is the largest, the growth crucible can be effectively supported and protected, meanwhile, the heat at the bottom of the growth crucible in the crystal growth process is timely extracted, and the damage of stress to the growth crucible is reduced, and meanwhile, a more stable and ideal crystal growth thermal field condition is established. The round angle can avoid the damage of the base to the growth crucible.
The invention has the beneficial effects that:
(1) the growth crucible is effectively fixed, and the growth crucible is prevented from moving left and right in the process of growing single crystals by a solution method; (2) the crystal growth crucible can be stably and closely supported, and the damage of stress to the growth crucible is reduced; (3) can extract heat in the crystal growth process in time, help to establish ideal crystal growth thermal field conditions, and stabilize the shape of a solid-liquid interface in the crystal growth process.
The invention adopts SiC with higher heat conductivity as the support material of the tellurium-zinc-cadmium crystal growth crucible, and timely extracts the heat in the tellurium-zinc-cadmium crystal in the growth process of the tellurium-zinc-cadmium crystal, thereby helping to establish ideal crystal growth thermal field conditions and stabilizing the form of a solid-liquid interface. The CdZnTe single crystal with the diameter of 90mm is successfully prepared by adopting the SiC support of the invention, and the single crystal rate and the quality of the crystal are greatly improved.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a top view of fig. 1.
Fig. 3 is a schematic view of cadmium zinc telluride ingot 1 in an embodiment of the present invention.
FIG. 4 is a schematic diagram of the deposition phases of cadmium zinc telluride ingot 1 in an example of the present invention.
In the figure: 1-a base substrate; 2-cambered surface groove; 3-round corner; 4-cylinder; 5-SiC powder.
Detailed Description
The technical scheme is described in detail with reference to the accompanying drawings and the detailed description.
As shown in figure 1, the SiC supporting holder for the growth crucible in the preparation process of the tellurium-zinc-cadmium crystal comprises a base body 1, wherein the base body 1 is a cylindrical growth crucible supporting holder prepared from a SiC material, the upper end face of the base body 1 is an arc-shaped groove 2 matched with the bottom surface of the growth crucible in shape, the outer diameter of a circle where the arc-shaped groove section of the smooth arc-shaped groove on the surface of the arc-shaped groove 2 is identical to the outer diameter of an equal-diameter section of the growth crucible, the inner diameter of the outer diameter of a seed crystal part of the growth crucible is slightly larger than the outer diameter of the seed crystal part of the growth crucible, the seed crystal part of the growth crucible can be embedded in the base body 1, and the concave surface of the arc-shaped groove 2 and the outer side of the base body 1 form a fillet 3 for transition. A cylinder 4 concentric with the base body is dug out from the lower end face of the base body 1 and used for being nested at the top end of a crystal growing rod of a crystal to ensure that a growth crucible is stably located at the center of a crystal growing furnace in the crystal growing process. The length of the base body is the same as that of the equal-diameter part of the growth crucible.
In actual operation, the SiC support with the cylinder 4 which is concentric with the base substrate 1 removed is embedded at the top end of the long crystal rod of the tellurium-zinc-cadmium crystal, the outer diameter of the long crystal rod is required to be the same as that of the cylinder 4, and the shaking effect is avoided in the crystal growth process. Then the growth crucible filled with the tellurium-zinc-cadmium material is placed on the arc-shaped groove 2, because the outer diameter of the arc-shaped circle on the interface of the arc-shaped groove 2 is the same as the outer diameter of the growth crucible, and the shape of the arc-shaped groove 2 is completely matched with the shape of the bottom surface of the growth crucible, the contact area between the arc-shaped groove 2 and the outer wall of the growth crucible is the largest, the growth crucible can be effectively supported and protected, meanwhile, the heat at the bottom of the growth crucible in the crystal growth process is timely extracted, and more stable and ideal crystal growth thermal field conditions are established while the damage of stress to the growth crucible is reduced. The round angle 3 can avoid the damage of the base to the growth crucible.
The embodiment provides a preparation method of a high-quality and large-diameter tellurium-zinc-cadmium single crystal, and SiC is selected as a support material of a tellurium-zinc-cadmium crystal growth crucible.
Example 1:
the first step is as follows: preparing materials and synthesizing according to the chemical metering ratio of the tellurium-zinc-cadmium crystal;
the second step is that: taking out the synthesized tellurium-zinc-cadmium polycrystal in a hundred-grade ultra-clean room, putting the polycrystal into a growth crucible, vacuumizing, and sealing and sintering the growth crucible;
the third step: placing the SiC support on a crystal growing rod in the crystal growing equipment of the vertical Bridgman method according to the actual operation;
the fourth step: placing the sealed and sintered growth crucible in the second step on the upper end surface of the SiC support in the third step, and growing the tellurium-zinc-cadmium crystal by a vertical Bridgman method;
the fifth step: taking out the growth crucible after the growth in the fourth step, taking out the tellurium-zinc-cadmium crystal ingot, and slicing on an inner circle slicing machine;
and a sixth step: after the cut CdZnTe wafer is polished, the deposition phase defect of the CdZnTe wafer is observed to be in a triangular Te-rich state under an infrared transmission microscope, and the density is less than or equal to 5 multiplied by 103cm-2

Claims (4)

1. A SiC support holder for a growth crucible in a tellurium-zinc-cadmium crystal preparation process comprises a base matrix (1), and is characterized in that:
the base body (1) is in a cylinder shape, and the upper end surface of the base body (1) is an arc groove (2) which is matched with the bottom surface of the growth crucible in shape;
the outer diameter of a circle where the arc section of the cambered surface groove (2) is located is the same as the outer diameter of the equal-diameter section of the growth crucible, the inner diameter of the arc section is larger than the outer diameter of the seed crystal section of the growth crucible, and the arc section is filled with SiC powder (5);
a fillet (3) is arranged between the concave surface of the cambered surface groove (2) and the outer side of the base body (1);
the lower end surface of the base body (1) is dug out a cylinder (4) concentric with the base body for being nested at the top end of a crystal growing long crystal rod.
2. The SiC support pedestal of claim 1, wherein:
the length of the base matrix (1) is the same as that of the equal-diameter part of the growth crucible.
3. The SiC support pedestal of claim 1, wherein:
the base body (1) is cylindrical.
4. The SiC support pedestal of any one of claims 1 to 3, wherein:
the SiC support is suitable for growing the tellurium-zinc-cadmium single crystal by a vertical Bridgman method and a vertical temperature gradient solidification method.
CN202011156052.XA 2020-10-26 2020-10-26 SiC support for growth crucible in tellurium-zinc-cadmium crystal preparation process Active CN114481288B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201883177U (en) * 2010-08-02 2011-06-29 北京博宇半导体工艺器皿技术有限公司 Crucible with BN (boron nitride)-silicon carbide composite structure for growth of compound semiconductor single crystal
JP2011251891A (en) * 2010-05-06 2011-12-15 Sumitomo Electric Ind Ltd Method for producing single crystal and crucible for single crystal production
CN103194790A (en) * 2013-04-03 2013-07-10 中山大学 Growth device and method for phosphorus-germanium-zinc single crystal
CN204982141U (en) * 2015-09-25 2016-01-20 大庆佳昌晶能信息材料有限公司 A PBN crucible unable adjustment base for single crystal preparation in -process
CN106757369A (en) * 2016-12-14 2017-05-31 中国科学院宁波材料技术与工程研究所 A kind of short warm area vertically moves stove and the method using its growth CdTe crystal
CN109252220A (en) * 2018-12-04 2019-01-22 中国电子科技集团公司第四十六研究所 A kind of VGF/VB arsenide gallium monocrystal furnace structure and growing method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011251891A (en) * 2010-05-06 2011-12-15 Sumitomo Electric Ind Ltd Method for producing single crystal and crucible for single crystal production
CN201883177U (en) * 2010-08-02 2011-06-29 北京博宇半导体工艺器皿技术有限公司 Crucible with BN (boron nitride)-silicon carbide composite structure for growth of compound semiconductor single crystal
CN103194790A (en) * 2013-04-03 2013-07-10 中山大学 Growth device and method for phosphorus-germanium-zinc single crystal
CN204982141U (en) * 2015-09-25 2016-01-20 大庆佳昌晶能信息材料有限公司 A PBN crucible unable adjustment base for single crystal preparation in -process
CN106757369A (en) * 2016-12-14 2017-05-31 中国科学院宁波材料技术与工程研究所 A kind of short warm area vertically moves stove and the method using its growth CdTe crystal
CN109252220A (en) * 2018-12-04 2019-01-22 中国电子科技集团公司第四十六研究所 A kind of VGF/VB arsenide gallium monocrystal furnace structure and growing method

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